HRID1443606

反应详情

EQUATION

反应方程式

HRID 1443606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 30 ml of ethylene glycol dimethyl ether, 8.4 g of 2,2,3,3,3-pentafluoropropyl trifluoromethanesulfonate and 5.9 g of malononitrile were dissolved. Thereto 12.3 g of potassium carbonate was added and the mixture was stirred at room temperature for 8 hours. Thereafter dilute hydrochloric acid was added to the reaction mixture and the mixture was extracted with t-butyl methyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 2.1 g of 2-(2,2,3,3,3-pentafluoropropyl)malononitrile.

WORKUP

后处理

  1. extractionthe mixture was extracted with t-butyl methyl ether
  2. washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure